摘要
目的建立准确适用的辣条中特丁基对苯二酚的2种测定方法,并对结果进行比较。方法优化国家标准中关于特丁基对苯二酚的提取、净化和液相色谱法,同时建立了辣条中特丁基对苯二酚的液相色谱串联质谱法,并对2种方法进行方法学验证,运用统计学比较2种方法测定结果的差异性。结果液相色谱法在5.0μg/ml~200.0μg/ml浓度内线性关系良好,检出限为3.0 mg/kg,不同浓度水平加标回收率为92.7%~98.3%,相对标准偏差(RSD)为0.9%~1.4%(n=6);液相色谱串联质谱法在1.0μg/ml~100.0μg/ml浓度内线性关系良好,检出限为1.5 mg/kg,不同浓度水平加标回收率为92.0%~98.6%,相对标准偏差(RSD)为0.8%~1.5%(n=6),2种方法测定结果差异无统计学意义(P>0.05)。结论优化后的提取效率高,净化效果好,高效液相色谱法结果更加准确可靠,建立的液相色谱串联质谱法灵敏度更高,选择性更强,2种检测方法均适用于辣条中特丁基对苯二酚的检验检测。
Objective To establish two accurate and applicable detection methods of tertiary butylhydroquinone in spicy strips and the results were compared.Methods The extraction,purification,high performance liquid chromatography(HPLC)of tertiary butylhydroquinone in the standard method was optimized.Meanwhile,a liquid chromatography tandem mass spectrometry(LC-MS)method for the determination of tertiary butylhydroquinone in spicy strips was established.The methodology verification was performed for the two methods.The difference between the two methods was compared statistically.Results The HPLC method had good linear relationship in the range of 5.0μg/ml-200.0μg/ml and the detection limit was 3.0 mg/kg.The recoveries of three spiked levels ranged from 92.7%to 98.3%with relative standard deviation of 0.9%-1.4%(n=6).The LC-MS method had good linear relationship in the range of 0.5μg/ml-15.0μg/ml and the detection limit was 0.5 mg/kg.The recoveries of three spiked levels ranged from 92.0%to 98.6%with relative standard deviation of 0.8%-1.5%(n=6).There was no statistical significance on the difference between the two methods(P>0.05).Conclusion The optimized method had good extraction and purification effect.The optimized HPLC method exhibited high reliability and accuracy.The newly developed LC-MS method was more sensitive and more selective.The two detection methods were suitable for the detection of tertiary butylhydroquinone in spicy strips.
作者
袁利杰
张培毅
秦逸飞
李彤辉
YUAN Li-Jie;ZHANG Pei-yi;QIN Yi-fei;LI Tong-hui(Henan Institute of Food Inspction,Zhengzhou,Henan 450003,China)
出处
《中国卫生检验杂志》
CAS
2021年第22期2705-2709,共5页
Chinese Journal of Health Laboratory Technology
基金
河南省市场监督管理局应用技术研究项目(2020sj36)。
关键词
辣条
特丁基对苯二酚
液相色谱法
液相色谱串联质谱法
Spicy strips
Tertiary butylhydroquinone
High performance liquid chromatography
Liquid chromatography tandem mass spectrometry
